Catalyst for synthesizing para-hydroxybenzenemethylal by using paracresol, preparation and use

A technology of p-hydroxybenzaldehyde and p-cresol, which is applied in the direction of oxidative preparation of carbonyl compounds, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of difficult recycling, poor product selectivity, Solve the problems of large separation load and achieve the effect of less by-products, low cost and easy separation

Inactive Publication Date: 2004-06-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a homogeneous catalyst, which is difficult to recycle and expensive, poor product selectivity, large separation load, and environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～6

[0020] Embodiment 1~6, preparation and evaluation of A series catalyst

Embodiment 1

[0022] Weigh 4.9g Co(NO 3 ) 2 .6H 2 O and 0.02gCu(NO 3 ) 2 .3H 2 O in a 250mL beaker to prepare a 120mL impregnation solution, and γ-Al 2 o 3 Add 100g carrier into the impregnating liquid, stir and mix well, after standing still for 24h, dry at 120°C for 12h, burn at 300°C for 3h, cool, grind finely, take 60-150 mesh size particles for evaluation, catalyst label is A-1 . The parameters for catalyst preparation are listed in Table 1.

[0023] In a 2.0L reaction kettle, the feeding amount is: 5.0g catalyst, 160.0g p-cresol, 500mL methanol, and 230g sodium hydroxide; seal the top of the kettle, stir and heat to 65°C, and react with oxygen, and the temperature rises and is controlled The reaction temperature is 75° C., and the reaction time is 120 minutes. Supplement oxygen intermittently to maintain the pressure in the kettle at 0.08-0.12MPa. After the reaction was completed, the reaction system was lowered to room temperature, the lid of the kettle was opened, and samp...

Embodiment 2

[0025] Weigh 100g γ-Al 2 o 3 The carrier was placed in a 500mL beaker, and 300mL of potassium hydroxide solution with a concentration of 0.01mol / L was added. After soaking for 24 hours, filter out the carrier, dry at 120°C for 12h, burn at 400°C for 3h, and cool for later use. Weigh 22.3gCo(NO 3 ) 2 .6H 2 O and 1.3g CuCl 2 .2H 2 O was prepared in a 250mL beaker to prepare 120mL of impregnating liquid, and the treated carrier was added to the impregnating liquid, stirred and mixed evenly, after standing still for 24h, dried at 120°C for 12h, burned at 500°C for 2h, cooled, ground into fine powder, and taken The particles with a size of 60-150 mesh were used for evaluation, and the catalyst designation was A-2. The parameters for catalyst preparation are listed in Table 1. Except that the catalyst is different, other reaction conditions and analysis methods are the same as in Example 1. The reaction results are shown in Table 1.

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PUM

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Abstract

The loaded catalyst for synthesizing p-hydroxybenzaldehyde is characterized by that the cobalt and copper are used as active component main agent, the atomic ratio of cobalt and copper is 1:0.05-1:10, one or several kinds of elements of iron, manganese, nickel, vanadium, zinc and cerium are used as active component adjuvant, the atomic ratio of total adjuvant and cobalt is 0:1-0.5:1, one of silica gel, titanium oxide and aluminium oxide or their composite material or active carbon can be used as carrier, the weight ratio of active component and carries is 0.01-0.3. The carrier is immersed into the solution containing said active component, dried, ignited and activated so as to obtain the invented catalyst. By action of said catalyst the p-hydrobenzaldehyde can be synthesized by direct oxidation of p-cresol.

Description

technical field [0001] The invention relates to the catalytic oxidation of p-cresol to synthesize p-hydroxybenzaldehyde, in particular to a catalyst for synthesizing p-hydroxybenzaldehyde from p-cresol, its preparation and application. Background technique [0002] p-Hydroxybenzaldehyde is an important intermediate in organic synthesis, and is widely used in medicine, fragrance, liquid crystal and pesticide industries. Such as the new generation of oral antibiotic sulfonamide synergist T.M.P, amoxicillin and amoxicillin cephalosporin, etc., as well as the synthesis of new heart disease drugs p-hydroxyphenylacetamide and hydroxyphenylglycine; in the fragrance industry, vanillin, syringaldehyde, Synthesis of anisyl alcohol, anisaldehyde and raspberry ketone, etc.; synthesis of new liquid crystal materials 4`-isopropyl-4-cyanobiphenyl, 1,2-bis(2-cyanophenoxy)ethane, etc.; New pesticides in pesticides, synthesis of herbicide intermediates, etc. [0003] The route of producing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/84B01J23/889C07C45/29C07C47/565
Inventor 徐杰王峰杨贯羽张伟吴文海
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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